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Synthesis and Characterization of [(C_5H_4SiMe_2~tBu)_2Ln(μ-S^nBu)]_2 (Ln=Y,Er)

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Chinese Journal of Structural Chemistry 2008年第5期27卷 523-528页

作者：李艳荣张正星陈珍霞刘瑞婷周锡庚 Department of Chemistry Molecular Catalysis and Innovative Material Laboratory Fudan University

（C5H4SiMe2^tBu）2Ln^nBu reacted with 1 equiv, of elemental sulfur in toluene at ambient temperature to yield the corresponding lanthanocene thiolates [（C5H4SiMe2^tBu）2Ln（μ-S^nBu）]2 （Ln = Y （1）, Er （2））. Complexes 1 and 2 have been characterized by elemental analysis, IR, mass spectroscopy and X-ray single-crystal diffraction analysis. Both complexes are of monoclinic with space group P21/c, formula C52H94S2Si4Y2 1 （C52H94S2Si4Er2 2） Mr = 1073.57 （1230.27）, a = 8.495（2）（8.41（2））, b = 26.913（8）（26.67（7））, c = 13.756（4）（13.68（4）） A, α = 90（90）, β = 101.184（5）（101.57（4））, γ = 90 （90）°, V= 3085.1（15）（3007（14）） A^3, Dc = 1.156 （1.359） g·cm^-3, Z= 2 （2）, F（000） = 1144 （1260）, μ = 2.046 （2.951） cm^-1, R = 0.0687 （0.0749） and wR = 0.1306 （0.1507） for observed reflections with I 〉 2σ（I）. X-ray structures of 1 and 2 definitively prove that only one sulfur atom is inserted into the Ln-C（^nBu） bond, forming a thiolate ligand.

关键词： organolanthanide crystal structure insertion elemental sulfur thiolate

Structural Evolution Patterns of FCC-Type Gold Nanoclusters

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物理化学学报 2018年第7期34卷 755-761页

作者： HIGAKI Tatsuya JIN Rongchao Department of Chemistry Carnegie Mellon University Pittsburgh Pennsylvania 15213 United States.

Recent progress in the research of atomically-precise metal nanoclusters has identified a series of exceptionally stable nanoclusters with specific chemical compositions. Structural determination on such "magic size" nanoclusters revealed a variety of unique structures such as decahedron, icosahedron, as well as hexagonal close packing(hcp) and body-centered cubic(bcc) packing arrangements in gold nanoclusters, which are largely different from the face-centered cubic(fcc) structure in conventional gold nanoparticles. The characteristic geometrical structures enable the nanoclusters to exhibit interesting properties, and these properties are in close correlation with their atomic structures according to the recent studies. Experimental and theoretical analyses have been applied in the structural identification aiming to clarify the universal principle in the structural evolution of nanoclusters. In this mini-review, we summarize recent studies on periodic structural evolution of fcc-based gold nanoclusters protected by thiolates. A series of nanoclusters exhibit one-dimensional growth along the [001] direction in a layer-by-layer manner from Au_(23)(TBBT)_(20) to Au_(36)(TBBT)_(24),Au_(44)(TBBT)_(28), and to Au_(52)(TBBT)_(32)(TBBT: 4-tert-butylbenzenethiolate). The optical properties of these nanoclusters also evolve periodically based on steady-state and ultrafast spectroscopy. In addition, two-dimensional growth from Au_(44)(TBBT)_(28) toward both [100] and [010] directions leads to the Au_(92)(TBBT)_(44) nanocluster, and the recently reported Au_(52)(PET)_(32)(PET: 2-phenylethanethiol) also follows this growth pattern with partial removal of the layer. Theoretical predictions of relevant fcc nanoclusters include Au_(60)(SCH_3)_(36), Au_(68)(SCH_3)_(40), Au_(76)(SCH_3)_(44), etc, for the continuation of 1 D growth pattern, as well as Au_(68)(SR)_(38)mediating the 2 D growth pattern from Au_(44)(TBBT)_(28) to Au_(92)(TBBT)_(44). Overall, this mini-review provides g

关键词： Gold Nanoclusters thiolate Face-centered-cubic Layer-by-layer growth

Structural Regularities of the Transition Metal Complexes Containing o-Benzenedithiol (H_2bdt)——Synthesis and Structure of Fe_3(bdt)_3(PBu_3~n)_3

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Science China Chemistry 1993年第8期36卷 912-919页

作者：康北笙徐勇进吴达旭彭金海洪茂椿翁林红陈学太刘汉钦 State Key Laboratory of Structural Chemistry and Fujian Institute of Research on the Structure of Matter Academia Sinica Fuzhou 350002 PRC

Complex Fe3（bdt）3（PBu3n）3 was synthesized in the presence of PBu3n and the structural regularities in a series of transition metal complexes containing bdtH2 ligand were summarized. The title complex crystallizes in the triclinic space group P-, Mr=1195.19, cell parameters: a=13.283（3）, b=20.115（5）, c=13.156（3）, （?）=90.33（2）, β= 116.47 （1）, γ=92.19（2）°, V=3143.5（2.7）3, Z=2, dc=1.26g/cm3. The structure was solved by direct methods from 4122 unique reflections with I>4σ（I） and reached the final convergence factor of R（Rw） = 0.053 （0.060）. The complex exhibits strong paramagnetism.

关键词： o-benzenedithiol ligand thiolate and phosphine-mixed coordinated complex structural regularity trinuclear iron cluster compound.

Synthesis and Thermal Stability of Antimony Tris (Thioethyl Stearate) for PVC

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Journal of Central South University 2000年第3期12卷 146-148页

作者： LIU You nian,WANG Chun jiang,SHU Wan gen,ZENG Dong ming,Chen Qi yuan (College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China) College of Chemistry and Chemical Engineering Central South University Changsha China

A novel type of thermal stabilizer antimony tris (thioethyl stearate)(ATS) was synthsized. Its thermal stability was measured by heat aging oven test when incorporated into PVC. ATS was synthesized from stearic acid, antimony trioxide and 2 mercaptoethanol in two steps. The reaction conditions of synthesis were optimized through orthogonal test. Experimental results show that the molar ratio of stearic acid and antimony tris (2 hydroxyethylthiolate) was 1.2, adding 0.6% tetra n butyl titanate as catalyst and xylene as azeotropic solvent, heating and refluxing for about 4 h, and the yield of ATS is 83.9%. The thermal stability time is about 40 min(at 200 ℃) when added 2phr(per hundred resin) in PVC. The thermal stability of ATS is better than that of Ca Zn complex and basic lead stabilizers, and equal to that of dibutyltin dilaurate.

关键词： thermal stabilizer antimony thiolate synthesis thermal stability

Synthesis and Structure of a Ruthenium(Ⅱ)-dithiocarbamate Complex [RuH(CO)(PPh_3)_2(4-ClPhNHCS_2)]·C_6H_(14)

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Chinese Journal of Structural Chemistry 2011年第4期30卷 470-473页

作者：王喜英史华田张千峰 Institute of Molecular Engineering and Applied Chemistry Anhui University of TechnologyMa'anshan

The title complex [RuH（CO）（PPh3）2（4-ClPhNHCS2）]·C6H14 has been prepared and characterized by X-ray diffraction *** crystallizes in the triclinic system,space group P1 with a = 11.0817（2）,b = 14.3889（2）,c = 15.2136（2） ,α = 71.018（1）,β = 74.911（1）,γ = 85.146（1）°,V = 2214.86（6） 3,Z = 2,Mr = 900.4,Dc = 1.350 g/cm3,Mr = 900.40,μ（MoKα） = 0.616 mm-1,F（000） = 926,S = 1.016,the final R = 0.0478 and wR = 0.0947 for 6828 observed reflections with I 2σ（I） and 505 *** molecular structure of 1 consists of one neutral complex [RuH（CO）（PPh3）2（4-ClPhNHCS2）] and one hexane solvent *** geometry around ruthenium is pseudo-octahedral with two trans-binding PPh3 ligands and one chelating bidentate 4-ClPhNHCS2- ligand via two sulfur *** average Ru-S,Ru-P and Ru-H bond lengths are 2.4824（8）,2.3495（8） and 1.71（2）,*** electrochemical properties of 1 have been studied in CH2Cl2 solution by cyclic voltammetry.

关键词： ruthenium dithiocarbamate thiolate hydride synthesis crystal structure

Synthesis and Crystal Structure of a Heterometallic Trinuclear Ni/Ag/S Compound

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Chinese Journal of Structural Chemistry 2012年第1期31卷 127-130页

作者：靳美亮马骁谭春红沈超君朱启龙胡胜民傅瑞标盛天录吴新涛 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterChinese Academy of Sciences

A new tri-nuclear mixed metal thiolate complex [Ag（PPh3）2]2[Ni（edtO2）2] 1 has been synthesized and structurally characterized by single-crystal *** molecule has a crystallographic inversion centre occupied in the central Ni（II） atom and the two silver（I） atoms are related by the inversion *** unique structural feature is that one of thiolates of each edt ligand has been oxidized to sulfinate from the precursor [Ni（edt）2]2-to the neutral linear trinuclear *** crystal structure belongs to the monoclinic system,space group P21/n with a = 13.581（11）,b = 12.239（9）,c = 22.316（17） ,β = 103.08（2）o,V = 3613（5） 3,Z = 2,Mr = 1571.87,Dc = 1.445 g/cm3,μ = 1.046 mm-1,F（000） = 1604,T = 293（2） K,the final R = 0.0652 and wR = 0.1499 for 6776 observed reflections with I 2σ（I）.

关键词： heterometallic chalcogenides thiolate chair-like crystal structure

[Co_3(1,2-S2C6H4)_3(PPh_3)_3]+, A basic triangle unit of some polynuclear molecules

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Chinese Journal of Chemistry 1994年第6期12卷 481-489页

作者： JIANG, Fei-Long HUANG, Xiao-Ying HONG, Mao-Chun CAO, RongWU, Da-Xu, LIU , Han-QinState Key Laboratory of Structural Chemistry and Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, China State Key Laboratory of Structural Chemistry and Fujian Institute of Research on the Structure of Matter. Chinese Academy of Sciences Fuzhou Fujian 350002 China

[Co3(1,2-S2C6H4)3(PPh3)3][CoBr3(DMF)].sol (1, sol=CHCl3,O(C2H5)2,H2O) was obtained from the reaction of CoBr(PPh3)3 with Na2(S2C6H4) in chloroform. The Co3 core in the cation of 1 exhibits a metal-metal bonded isosceles triangle, in which the two longer Co-Co bonds are both bridged by S2C6H4 ligands on two sides of the triangle plane respectively, while the bottom short Co-Co bond is bridged by the third bidentate S2C6H4 ligand. A series of polynu-clear cobalt cluster compounds with phosphine, thiolate and/or sulphur ligands were prepared by low oxidation state Co+ with thiolates in organic solvents. These tri-, tetra-, hexa-, heptanuclear cluster compounds 1-8 with various types of crystal structures can be viewed as the condensed polynuclear cobalt complexes that the cobalt atom frameworks with sulphur bridged were built through the small triangular units of [Co3S3nL3] (n=1,2) with or without [CoL] (L=PR3, Br, Cl, 5-C5H5) fragments.

关键词： Polynuclear cobalt thiolate phosphine structure.